No abstract

A rapid, specific and sensitive ultra-performance liquid chromatography tandem mass spectrometry method was developed for the determination of fenofibric acid in human plasma. The method involves simple, one-step liquid-liquid extraction procedure coupled with an Acquity UPLC(TM) BEH C(18) column (50 x 2.1 mm, i.d., 1.7 microm) with isocratic elution at a flow-rate of 0.2 mL/min and mefenamic acid was used as the internal standard. The Quattro Premier XE mass spectrometry was operated under the multiple reaction-monitoring mode using the electrospray ionization technique. Using 250 microL plasma, the methods were validated over the concentration rang 0.05-7.129 microg/mL, with a lower limit of quantification of 0.05 microg/mL. The intra- and inter-day precision and accuracy were within 9.3%. The recovery was 66.7% and 52.6% for fenofibric acid, and mefenamic acid, respectively. Total run time was 1.8 min only for each sample, which makes it possible to analyze more than 350 samples per day.

A method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) in combination with solid-phase extraction for sample pretreatment has been developed for the simultaneous analysis of amitriptyline and its main metabolite in human plasma. The extraction of the analytes from plasma samples was carried out by means of a selective SPE procedure using hydrophilic-lipophilic balance cartridges. The assay involves a simple solid-phase extraction (SPE) procedure of 0.2 mL of human plasma and analysis was performed on a triple-quadrupole tandem mass spectrometer by multiple reactions monitoring (MRM) mode via electrospray ionization (ESI). The standard calibration curve was linear over the ranges 0.370-95.539 ng/mL for amitriptyline and 0.365-94.374 ng/mL for nortriptyline, expressed by the linear correlation coefficient r², which was better than 0.995 for both. The intra- and inter-day precision and accuracy of the quality control samples were within 10.0%. The recovery was 85.3, 88.4 and 80.7% for amitriptyline, nortriptyline and doxepin respectively. Total run time was 1.2 min only for each sample, which makes it possible to analyze more than 400 samples per day. The method was highly reproducible and gave peaks with excellent chromatography properties.

A rapid and sensitive ultraperformance liquid chromatography tandem mass spectrometry assay was developed for the simultaneous analysis of oxcarbazepine and its main metabolite in human plasma. The assay involves a simple solid-phase extraction procedure of 0.3 mL of human plasma and analysis was performed on a triple-quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionization. Separation was achieved on an Acquity UPLC™ BEH C₁₈ column (50 × 2.1 mm, i.d., 1.7 µm) with isocratic elution at a flow-rate of 0.25 mL/min and imipramine was used as the internal standard. The standard calibration curve was linear over the range 9.580-5070.205 ng/mL for oxcarbazepine (OXC) and 19.444-10290.800 ng/mL for 10,11-dihydro-10-hydroxycarbamazepine (MHD), expressed by the linear correlation coefficient r², which was better than 0.995 for OXC and MHD. The intra- and inter-day precision and accuracy of the quality control samples were within 10.0%. The recoveries were 81.0, 89.6 and 66.6% for OXC, MHD and imipramine, respectively. The total run time was 1.5 min only for each sample, which makes it possible to analyze more than 350 samples per day.

A novel, specific and sensitive ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/ MS) method was developed for the simultaneous determination of quinapril and its active metabolite quinaprilat in human plasma. The method involves a simple, one-step extraction procedure coupled with an Acquity UPLC TM BEH C 18 column (100 × 2.1 mm, i.d., 1.7 mm) with isocratic elution at a flow-rate of 0.2 mL/min and lisinopril as the internal standard. Detection was performed on a triple-quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionization. Using 250 mL plasma, the methods were validated over the concentration range 5.010-500.374 ng/mL for quinapril and 10.012-1000 ng/mL for quinaprilat, with a lower limit of quantification of 5.010 ng/mL for quinapril and 10.012 ng/mL for quinaprilat. The intra-and inter-day precision and accuracy were within 10.0%. The recovery was 85.8, 62.6 and 61.3% for quinapril, quinaprilat and lisinopril, respectively. Total run time was 3.0 min only.